CN101156835B - Preparation method of hypericin oral liquid - Google Patents
Preparation method of hypericin oral liquid Download PDFInfo
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- CN101156835B CN101156835B CN2007101229126A CN200710122912A CN101156835B CN 101156835 B CN101156835 B CN 101156835B CN 2007101229126 A CN2007101229126 A CN 2007101229126A CN 200710122912 A CN200710122912 A CN 200710122912A CN 101156835 B CN101156835 B CN 101156835B
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- hypericin
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Abstract
The invention relates to a preparation method of hypericinoral oral liquid, which belongs to the medicament preparation field. The preparation of the applied hypericinoral Chinese medicine agent at present is relatively complicated, the usage is not convenient, the invention prepares the hypericinoral into the oral liquid, 40-120 g hypericinoral extracturm is added in the 70-160 ml double solvent, and then the hypericinoral extracturm is agitated, compound solvent comprises tween minus 80:1 and propylene glycol is 2: 1, the prepared oral liquid improves the stability and the water solubility of the hypericinoral, the route of medication is changed, the invention is favor of clinical usage, the mouth feel is improved, the absorption of medication is increased, and the preparation process is simple, the operation is easy, and the invention is favor of generalization.
Description
Technical field
The present invention relates to the medicament preparation field, especially the preparation method of oral liquid.
Background technology
Hypericin (hypericin4,4,5,5,7,7-hexahydroxy-2,2-dimethyl-meta-meso-naphthadianthrene ketone) molecular formula is C
30H
16O
8, molecular weight is 504.43, is the material of biologically active among the Herba Hyperici perforati Hypericum perforatum L., has antidepressant, calmness, anti-inflammation, especially antivirus action is outstanding, can anti-DNA, RNA viruses.Studies show that to have very strong antivirus action by Lanzhou herding and veterinary drug institute extraction separation and synthetic hypericin complex from Herba Hyperici perforati.Present hypericin is to produce with the form of the Chinese medicine preparation of Herba Hyperici perforati, and this has limited the performance of curative effect, uses also inconvenience.The present invention studies oral liquid, preparation technology to hypericin oral liquid compares, therefrom select a kind of best preparation technology, and require its quality standard is studied, so that hypericin oral liquid is further promoted clinical application research according to Chinese Pharmacopoeia.
Summary of the invention
Purpose of the present invention is for providing a kind of technology simple, the preparation method of the hypericin oral liquid of stable content.
The technical scheme that realizes above-mentioned purpose is as follows:
The preparation method of hypericin oral liquid is to add double solvents 70-160ml among the hypericin extractum 40-120g that makes with prior art, adds the entry standardize solution again and stirs to 300ml.Consisting of of double solvents: tween 80: 1,2 propylene glycol=2:1.
The hypericin oral liquid that is made by technique scheme carries out the hypericin Determination on content, and step is as follows:
1, the preparation of need testing solution:
Draw the hypericin oral liquid that has prepared, extract with ethyl acetate, get the 200ml oral liquid for the first time and extract, get the above-mentioned liquid 150ml that has extracted for the second time, extract again, get the liquid 100ml of extraction last time after for the third time at every turn, extract again, orange redly in the extraction phase weaken gradually, in the time of the 7th time, color is near colourless in the extraction phase, and thin layer chromatography detects, and the fluorescent red-orange speckle is extremely faint, stop extraction, combining extraction liquid, Rotary Evaporators distilling under reduced pressure under 50 ℃ of conditions is scraped the gained hypericin in the brown bottle and to be kept in Dark Place, during obtain solution, precision takes by weighing hypericin 0.1mg, puts in the 10ml volumetric flask, adds dissolve with methanol, and be settled to scale, shake up, filter, promptly join to such an extent that concentration is the need testing solution of 0.01mg/ml with 0.45 μ m filter.
2, the preparation of reference substance solution:
The hypericin that utilizes the production of Sigma company is as standard substance.Precision takes by weighing hypericin standard substance 0.1mg, puts in the volumetric flask of 10ml, adds dissolve with methanol and be settled to scale to shake up, and filters with 0.45 μ m filter and promptly joins to such an extent that concentration is the standard solution of 0.01mg/ml.
3, thin layer is identified:
With the test sample that ethyl acetate extracts, selecting developing solvent for use is petroleum ether-ethyl acetate-methanol (2:8:3), and after solvent launched, taking-up was dried, and inspects to be orange-red fluorescence speckle under uviol lamp (254nm), compares R with standard substance
fValue.
4, check result:
Character: this product is the blush transparency liquid, odorless, mildly bitter flavor.
Resin is checked: sample thief 5ml adds 1 of hydrochloric acid, observes no resin-like thing after half an hour and separates out (press 2005 editions " inspection of Chinese pharmacopoeia appendix inspection technique), and is up to specification.
Hemolytic test: " inspection of Chinese pharmacopoeia appendix inspection technique should be up to specification to press 2005 editions.
Adopt the content of high performance liquid chromatography test sample:
Testing conditions: chromatographic column: KromasilC18 (250mm * 4.6mm, 5 μ m).
Mobile phase: acetonitrile-distilled water (140:10 includes 1% glacial acetic acid).
30 ℃ of column temperatures.
Flow velocity 1ml/min.
Detect wavelength: 284nm.
The drafting of standard curve: the hypericin reference substance solution sample introduction of drawing 0.2 μ l, 0.4 μ l, 0.6 μ l, 0.8 μ l, 1.25 μ l respectively, measure the standard curve of sample size and peak area. is the standard curve of abscissa with peak area Y to its sample size X (μ l), and standard curve is seen Fig. 1.
The linear relationship that records standard curve is good, and the gained regression equation is y=1.64 * 10
6X-96901R=0.9990
When calculating the content of hypericin, the peak area of working sample at first is the hypericin content of institute's test sample product again from the X value of the corresponding point correspondence of standard curve.
Stability experiment:
The hypericin less stable must be preserved under the condition of low temperature, black out.But hypericin is made into oral liquid, has improved the water solublity of hypericin.The placement of hypericin oral liquid preparation after 15 days, is observed the variation of its outward appearance and content.
The result shows: hypericin oral liquid is not found any variation of outward appearance after placing 15 days, promptly keep original aubergine, bright, do not have a sedimentary outward appearance.The stability that hypericin oral liquid is described strengthens greatly than hypericin, makes clinical practice more convenient.
The accurate reference substance solution 20 μ l that draw divide equally sample introduction every 2h in 24h, measure 12 times down by " drafting of standard curve " item.The result is that to record peak area 12 times constant substantially, RSD=1.37% (n=12).Stability is in allowed band.
The precision experiment:
Get the hypericin reference substance solution, distinguish 6 hypericin Determination on content of sample introduction, record the content RSD=1.02% of hypericin.Precision is in allowed band.
Proved that by hypericin assay in the above-mentioned control sample precision of Stability of Hypericin and method is measured in the oral liquid, and then the method for testing that has proved hypericin content is: satisfy test requirements document, and can be as method of testing for test agent.
Assay for hypericin in the test agent
Each accurate the absorption for test agent liquid 20 μ l sample introductions, the peak area according to the condition determination working sample of standard substance calculates content.The results are shown in Table 1 and Fig. 2, Fig. 3
Table 1 hypericin injection assay
| The injection lot number | The average content of hypericin (mg/ml) | Meansigma methods (mg/ml) | RSD(％) |
| 20C60817 | 0.0092 | ||
| 20C60818 | 0.0094 | 0.0093 | 1.07％ |
| 20C60822 | 0.0093 |
More than the content of hypericin is stable in the high effective liquid chromatography for measuring oral liquid of Cai Yonging, accurately and reliably.The hypericin oral liquid that draws the present invention's preparation from above data is successful, and this will further promote the exploitation and the clinical practice of hypericin.
The present invention also has following beneficial effect:
1, improved the water solublity of hypericin.
2, change the route of administration of hypericin, made things convenient for the use in veterinary clinic.
3, because ill domestic animal generally has appetite depression, even the refusing to eat phenomenon is arranged, and hypericin oral liquid can change the palatability of animal, increases the absorption of medicine, has improved availability, has reached the effect of moisturizing simultaneously.
4, simple, the processing ease of technology, be convenient to promote.
Description of drawings:
Fig. 1 is the standard curve of hypericin content and chromatographic peak area
Fig. 2 is the high-efficient liquid phase chromatogram of hypericin control sample
Fig. 3 is the high-efficient liquid phase chromatogram of hypericin for test agent
The specific embodiment
By the embodiment shown in 2 that tabulates down technical scheme of the present invention is described further.
The embodiment of table 2 hypericin oral liquid
More than the hypericin oral liquid of each embodiment manufacturing can both reach stable content, accurately and reliably, be suitable for the medicament of clinical practice.
Claims (1)
1. the preparation method of hypericin oral liquid is characterized by add double solvents 70-160ml in hypericin extractum 40-120g, adds that water is fixed molten to stir to 300ml again, the consisting of of described double solvents: tween 80: 1,2 propylene glycol=2:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101229126A CN101156835B (en) | 2007-07-03 | 2007-07-03 | Preparation method of hypericin oral liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101229126A CN101156835B (en) | 2007-07-03 | 2007-07-03 | Preparation method of hypericin oral liquid |
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| Publication Number | Publication Date |
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| CN101156835A CN101156835A (en) | 2008-04-09 |
| CN101156835B true CN101156835B (en) | 2010-10-06 |
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| CN2007101229126A Expired - Fee Related CN101156835B (en) | 2007-07-03 | 2007-07-03 | Preparation method of hypericin oral liquid |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101744795B (en) * | 2010-03-11 | 2012-07-04 | 中国人民解放军第三军医大学第三附属医院 | Medicinal composition for treating nevus flammeus and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1408396A (en) * | 2001-09-25 | 2003-04-09 | 北京北大维信生物科技有限公司 | Jinyukang-oral medicine for curing depression |
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2007
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1408396A (en) * | 2001-09-25 | 2003-04-09 | 北京北大维信生物科技有限公司 | Jinyukang-oral medicine for curing depression |
Non-Patent Citations (3)
| Title |
|---|
| 李海燕.龙芩草、通络救脑组方成分的药学、药效学及作用机制.北京中医药大学博士研究生学位论文.2006,第90页3.1.3.1-3.1.3.2. * |
| 王娥.口服制剂中增溶辅料的研究进展.医药导报25 9.2006,25(9),934-936. |
| 王娥.口服制剂中增溶辅料的研究进展.医药导报25 9.2006,25(9),934-936. * |
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Granted publication date: 20101006 Termination date: 20110703 |